反应详情

A solution of 105 mg (0.31 mmol) of 2,2-difluoro-2-(2-pyridyl)ethyl trifluoromethanesulfonate and 43 mg (0.66 mmol) of sodium azide in 1.0 ml of DMF was heated at 60° C. After 1.5 h, the mixture was cooled, diluted with water and extracted with two portions of ether. The combined organic layers were washed twice with water, brine and dried over MgSO4. The solvents were removed at reduced pressure to give 1-9 as a brown oil: 1H NMR (CDCl3) δ8.68 (d, 1H, 4.2 Hz), 7.86 (td,1H, 7.8, 1.5 Hz), 7.72 (d, 1H, 7.8 Hz), 7.40-7.45 (m, 1H), 4.03 (t, 2 H, 13.2 Hz).

1. temperaturethe mixture was cooled
2. extractionextracted with two portions of ether
3. washThe combined organic layers were washed twice with water, brine
4. dry with materialdried over MgSO4
5. customThe solvents were removed at reduced pressure